原创《中心切割二维液相色谱串联质谱法分析烟草农残》：这篇液相色谱论文范文为免费优秀学术论文范文,可用于相关写作参考。
摘 要：开发了中心切割二维液相色谱/串联质谱联用分析烟草多种农药残留的技术.该方法采用二维液相色谱串联质谱,第一维体积排阻色谱和第二维反相液相色谱通过定量环进行转移.第一维的体积排阻色谱分离去除大分子物质,目标馏分经分流后切割至六通阀上的定量环.目标物收集完成时通过阀转动第二维流动相将目标物带入第二维反相液相色谱进一步分离.运用质谱的多反应监测模式（multi reaction monitoring, MRM）对74种农残进行定性定量分析,检测结果和一维LC-MS/MS方法较为一致,农药回收率72%～136%,定量限0.022～0.152 mg/kg.研究开发的中心切割多维液相色谱/串联质谱联用测定烟草农残方法可由仪器自动运行,结果准确可靠,适合于大量烟草样品多组分农残的自动分析检测.
关键词：农残；烟草；二维液相色谱；中心切割
中图分类号：S435.72 文章编号：1007-5119（2017）06-0041-07 DOI：10.13496/j.issn.1007-5119.2017.06.006
Abstract： A new concept for sample cleanup, based on size exclusion of macro molecular compounds in matrix, has been developed by coupling of gel permation chromatography （GPC） with LC-MS/MS. Heart-cutting two-dimensional liquid chromatography tandem mass spectrometry system was used by transferring the target elution through a loop. In the two dimensional liquid chromatography -tandem mass spectrometry system, a GPC column was employed in the first dimension to separate the macromolecule interference compound weight. After split, the target fluent were heart-cutting to a loop connected to a 6-way valve. Then the valve switched, so the second dimensional mobile phase took the target compounds for further reversed phase liquid chromatographic separation. Finally, about 80 different species of pesticide residues were determined qualitatively and quantitatively under the multi reaction monitoring （MRM） mode. The recoveries of most pesticides were in the range of 72%-136% and the limits of quantitation （LODs） for this method were from 0.022 to 0.152 mg/kg. Compared to conventional approaches for pesticide residue analysis in tobacco, the new technique involves less contamination of ion source in MS without sacrificing method LODs. In addition, the 2DLC-MS/MS method was fully automatic and the results were also accurate when utilized to detection of tobacco samples.
Keywords： pesticide residues； tobacco； two dimensional liquid chromatography； heart-cutting
烟草作为世界上种植最广泛的非粮食作物,在全世界129个国家和地区种植[1].在烟草栽培、生长、成熟和储存醇化过程中,常需要农药[2],因此,农药残留作为烟草质量安全问题的一个重要组成部分,引起广泛关注[3-4].國际烟草科学研究合作中心（CORESTA）于2003年首次提出烟草中农用化学品指导性残留限量（Guidance Residue Levels, GRLs）,至2016年已经更新至第四版,涉及农药从最初的99种增至106种[5].
有关农药残留检测的研究一直是CORESTA会议关注的热点[6],行业内出台了相应的检测标准[7-8],常用的方法主要有GC-MS/MS和LC-MS/MS方法.CHEN等[9]建立了GC-MS/MS测定烟草中159种农药残留的方法,并将其用于118种不同烟草样品的 测试.KERKDIJK[10],GUO[11],LU等[12]运用GPC、SPE和GC-MS相连等技术净化样品,从而达到减少基质效应的效果.QI等[13]采用在线LC-GC技术,测定了18种有机氯农残.LC-MS/MS法测定农药残留量近年来得到了广泛应用[14-16],BERNARDI等[15]报道采用低温和分散微萃取技术净化样品,并进行LC-MS/MS测定.
液相色谱论文参考资料：
结论：中心切割二维液相色谱串联质谱法分析烟草农残为关于液相色谱方面的的相关大学硕士和相关本科毕业论文以及相关液相色谱使用方法论文开题报告范文和职称论文写作参考文献资料下载。
